Sulfur heterocycles are found in low concentrations in most coalderived liquids and shale oils, and therefore, isolation of the heterocyclic sulfur fraction is necessary for individual compound Identification. In this report, a new methodology for the isolation and subsequent separation and identification of sulfur heterocycles is described and applied to selected coal liquids and shale oils. Identification was accomplished by sulfur-selective flame photometrk detection and comparison of mass spectral and chromatographic retention data of mixture components with standard reference compounds. Chromatographic retention data for 32 standard sulfur heterocycles were determined.

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The synthesis of dinaphtho[1,2‐b:2′,3′‐d]thiophene (6), dinaphtho[2,1‐b:2′,3′‐d]thiophene (15), dinaphtho‐[1,2‐b:1′,2′‐d]thiophene (20), dinaphtho[2,1‐b:1′,2′‐d]thiophene (26), dinaphtho[2,3‐b:2′,3′‐d]thiophene (37) and dinaphtho[1,2‐b:2′,1′‐d]thiophene (45) has been accomplished.

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